Automatic sample cutter



J n- 1954 T. R. MARCELL arm.

AUTOMATIC SAMPLE CUTTER 5 Sheets-Sheet 1 Filed Nov. 16, 1951 vacuum PUMP GLPSS IIIIII/IIII/IIIIIII IIIIIII/Il Hea d; Uni? Jan. 1 54 T. R. MARCELL ETAL AUTOMATIC SAMPLE CUTTER 5 sheets-sheet 2 Filed NOV. 16, 1951 E 729622 7% 1079 Car Jan. 12, 1954 1- MARCELL r 2,665,585

AUTOMATIC SAMPLE CUTTER Filed Nov. 16 1951 5 Sheets-Sheet 3 6] OPEN) OPEN (oFF) swe u a 12, 1954 T. MARCELL arm. 2,665,585

AUTOMATIC SAMPLE CUTTER Filed NOV. 16, 1951 5 Sheets-Sheet 4 Jan. 12, 1954 T. R. MARCELL ETAL AUTOMATIC SAMPLE CUTTER Filed Nov. 16, 1951 5 Sheets-Sheet 5 Patented Jan. 12, 1954 AUTOMATIC SAMPLE CUTTER,

Thaddeus R. Marcell and Carter E. Porten Cranford, and John H. Staib, Scotch Plains, N J.

5 Application November 16, 1951, Serial No. 256,662

This invention relates to sample cutters such as are employed in connection with research laboratory apparatus for fractional distillation of hy drocarbon fuels for the purpose of taking therefrom test samples of the distillate at intervals controlled by time, volume of fraction, or temperature change.

As is well known to persons skilled in the abovecited art to which the invention is particularly applicable, liquid hydrocarbon fuel is raised to the boiling point in a still pot located at the base of a vertical distillation column. Vapor from the boiling liquid rises in the column to varying heights, condenses into the liquid state, and flows back into the still pot. The most volatile components, i. e. those having the lowest boiling point, concentrate at the top of the column and it is these fractions from which it is most desirable to obtain cuts for test purposes, so a cooling jacket is provided surrounding the top portion of the distillation column to accelerate condensation at this point. At predetermined intervals, distillate from the top portion of the column is diverted into an exteriorly located collector, which also has a cooling jacket. In order to lower the temperature at which the liquid contents of the still pot will boil and thereby insure safe distillation without danger of cracking or burning, the pressure in the apparatus is reduced to a suitable degree below that of atmospheric distillation by 9 Claims. (Cl. 73-422 has accumulated in the collector, it is drawn tifiable receivers. We are also aware of a sample cutter invented by another which is automatic in-operation. That device has a rotatable frame or rack which holds a great many vertically dis- .posed sample tubes that are arranged in concentric circular rows. A filling tube connected with the drainage duct of the distillation apparatus is swingable on a vertical axis so that its lower discharge end may overlie each receiver of the series in turn as the rack is intermittently rotated. After all receiversof one row are filled,

a cam plate swings the discharge end of the filling tube over to the next row. This operation continues until the last empty receiver has been filled, whereupon the filling tube is displaced into registration with a discharge opening in the rack 40*means by which an operator may interpose irregand the motion of the latter is stopped. This, automatic sample cutter was devised to reduce manual control to a minimum and even to permit unattended operation at night or on week-ends. It has numerous defects, however, among which the most serious are: (1) there is no control ofthe flow of distillate into or through the filling'tube, so there will be spilling of liquid during the interval when the rack moves to bringa fresh sample receiver into registration with said"tub'e; (2) all sample receivers are open to the atmosphere, so wasteful and dangerous evaporation of inflammable material will occur, which is particularly serious during those long periods when the device is unattended; (3) there is no provision for restoration of the associated distillation column to total reflux condition upon cessation of operation of the sample cutter; and, (4) the device cannot be made to operate successfullywith distillation apparatus which has its internal pressure reduced below that of atmospheric distillation, for the distillate will not flow from the collector into the filling tube of the sample cutter.

With the above-enumerated defects of theprior art apparatus in mind, it is our primary object to provide an improved automatic sample cutter which shuts off the flow of distillate before each shift of the filling tube or conduit from one sample receiver to the next one in the series, which restores the distillation apparatus to total reflux condition and suspends all operation of the moving parts of the sample cutter immediately following delivery of a sample cut into the final receiver of the series, and which seals the sample receivers from the atmosphere either after receiving their samples in one embodiment of the invention or continuously in another embodiment.

"Another object of the invention is to provide ular manual operation of the filling conduit'shifting means and the control valve of' the distillation apparatus to permit the taking of a casual sample out under unusual circumstances. Further objects and advantages of the invention should become apparent as the following specific description is read in conjunction with the accompanying drawings, in which:

Fig. l is a small-scale diagrammatic view, partly in section, of a typical fractional distillation apparatus of the reduced-pressure or vacuum type, showing the preferred form of automatic sample cutter applied thereto; Fig. 2 is an enlarged perspective view, partly broken'away, of

the preferred form of automatic sample cutter .should be kept under visual observation automatically at the end of a major cycle of operation; Fig. is a similar view -showing .commencement of the first minor cycle of operation within a major cycle; Fig. "6 a similar view,

showing the next stage of operation of the first minor cycle; Fig. 7 is a similar view, showing a later stage of said first minor cycle; .and Fig. 8 is a similar view, showing completion of the first minor cycle with the shut-down switch and total reflux restoration switch in broken line positions representing precise termination of a major cycle.

Fig. ,9 is a plan view or" a modified form of sample cutter, showing the filling conduit memberat an intermediate position in the major cycle of operation; Fig. 10 is a fragmentary elevational view of the same, partlyinsection; .and Fig. 11 is adetail exploded side elevation of a sample receiver and holder, the latter being broken away.

Before proceeding with description of the specific structural details of the invention, it should bemade clear that the invention has other useful applications outside the art of fractional distillation of hydrocarbon fuels. In the various industrial arts, there are chemical processes and qualitative treatment of liquids and solids in granular or pulverulent 'form in the course of which the employment .of an automatic sample cutter such as ours will fill a real need. In the accompanying drawings, the invention is represented in ,its adaptation to a typical distillation apparatus, but it will be understood that it is intended to cover all adaptations, changes and modifications of the examples of the invention ,herein chosen for the purpose of illustration whichdo not constitute departures from the spirit of the invention.

' Because, in .the adaptation of the invention to anapparatus foriractional distillation of hydrocarbon fuels, .certain elements of the formerenter into close cooperative relation with elements of the.latter,conventional-disclosure of a typical distillation apparatus has been included. In this connection, letters have .been used to indicate old orstandard elements, whereas numerals refer to that which is believed to be new.

Referring now to the drawings, in whichlike reference characters designate corresponding parts in the several views, Fig. lshows the typical distillation apparatus with thesamplecuttermechanically and electrically connected thereto for operational use therewith. It will be observed that a vertical distillation column .A communicates at its base with a still pot .B. The upper .end portion of columnA iscooled by an external water jacket C. Column A and still .pot B usually :are made of glass and are integrally formed.

Glass customarily is used for any other structural elements which mayoontain liquids which Immediately below water jacket C, there is flow diversion means comprising a fixed funnel -D -formed centrally in :column ,A and a swinging funnel E, which is pivotally mounted in column A close beneath funnel D to receive the descending flow of condensed vapor directed into it by said fixed funnel and which, when tilted into the position disclosed in Fig. 1, will divert the downfiowing distillate into a trough F that drains into a duct G leading exteriorly downward from column A into acollector I-I. Swinging funnel E may be made of glass but must include in its structure a suitable mass of magnetic material, such as iron, ior cooperation with an exteriorly located electromagnet I which may be energized periodically by electric current through the medium of circuit J. .The said circuit is controlled by a suitable timer T, which may be set to energize electromagnet I in accordance with a predetermined time ratio.,.-such as for three seconds in every twenty seconds. When electromagnet I is ener gized, it draws the spout of swinging funnel E over into the position shown, wherein all descending distillate from fixed funnel D will be drawn off into collector H. When the circuit is'bro'ken at the end of the predetermined time period, swinging funnel E will gravitate into upright position wherein all distillate entering said funnel from then until electromagnet becomes energized again will be directed past trough F into the lower portion of column A for return to still pct 13. This intermittent return, or reflux, of distillate from the top portion of column A is opposed to-the total reflux condition which obtains when timer T is not in operation or circuit J is opened and swinging funnel becomes immobilized in its normal upright position.

Timer T is manually adjustable to vary the time ratio for diversion of distillate cuts into collector H. In addition to this normal-control of distillate diversion, a secondary circuit Win-series with circuit J is provided for connection with secondary control means which forms part of the electrical operating means of the preferred embodiment of our automatic sample cutter, which is shown in Figs. 51 to 8 inclusive, and will be described in detail presently.

Collector H, which usually is also provided with a cooling water jacket L, has a downwardly directed drainage duct that may be controlled by a solenoid-actuated valve N. An extension drainageduct 22 leads from valve N downwardly for operative connection with the sample cutter in amanner which will be understood when details of the latter are described. In further adaptation of the distillation apparatus'to cooperative solenoid valve N'is extended to said sample cutter forconnection with the appropriate circuit of the electro-mechanical operating mechanism thereof.

It has already been mentioned that operation of the distillation apparatus can be carried .out with comparative safety by reducing the internal pressure below that of atmospheric distillation. In order to obtain this condition, it is the usual practice to connect the upper end of distillation column A with a vacuum pump by a tubular main vacuum line O. Then, to equalize the pressure throughout the apparatus, a branch vacuum line jP interconnects main line 0 and the upper end of collector H, and. another branch line 23, having a manuallyoperable shut-off valve 23a and a lower valve .231) controlling atmospheric vent 2'30, .ex-

The preferred embodiment of the sample cutter, which is intended for use with distillation apparatus of the reduced-pressure type, is illustrated in Figs. 1, 2, 3, and 4 to 8, inclusive. The

principal components of the device are: (1) the supportingstructure 24; (2) the holding means 25 for sample receivers 25; (3) filling conduit holders 25 being stationary; (5) envelope 29'to *seal the interiors of sample receivers 26 and the various ducts and vessels of the distillation apparatus from the atmosphere; and (6) the electro-mechanical operating mechanism, preferably housed in supporting structure 24, which in mutual cooperative relation to the distillation apparatus motivates power transmission means 28 and coordinates its movement with the timed draining of sample cuts or fractions from the distillation apparatus and with the control of the swinging funnel E of the latter.

Supporting structure 24 may take any desired general form but preferably comprises a base 24a,

standard 241) rising from said base, and horizontal armz lc projecting from standard 24b. Standard 24b is box-like in structure for the purpose of housing the operating mechanism.

Sealing envelope 29 preferably is semi-spherical in form and has a top neck 3| which is removably secured in stationary position in supported relation to arm 240 of supporting structure 24 by any suitable means, such as by clamp 3'2. It

'is desirable to make envelope 29 of glass for reasons which should be obvious to those skilled in the art. The bottom wall 'of said envelope is upthrust into exteriorly concave form as at 33 and merges with the side walls in an annular channel from which regularly spaced spout-form holders 25 for sample receivers 26 project downward.

Holders 25 preferably are tapered toward their "free ends to fit the mated flared necks 26 of receivers 26. Due to the glass composition of envelope and receivers, the mated abutting outer and inner surfaces, respectively, of holders 25 and receiver necks 26 may be ground in accordance with common practice to effect a fluid-tight joint. By providing downwardly raking hooks 34 on I the necks 26' of receivers 26, it is convenient to apply closing pressure to said joint at each holder 7 by means of a securing device 35, which may be in the form of the spring loop shown. Each securing device 35 is attached in suitable manner to envelope 29, as by integral perforate lug 36, and is adapted to be engaged with the hook 34 of H any sample receiver 26 applied to the corresponding holder 25 after said securing device has been stretched into highly tensioned condition. The size and tension of the loop should be such that, securing device 35 will exert a strong upward pull on the receiver. To facilitate manipulation of each securing device 35, it is preferred to provide a pendant flexible member 31, such as a chain,

having a finger ring 38 at its free end.

When all holders 25 have sample receivers 26 operatively applied thereto, the bottom and side areas of envelope 29 will be hermetically sealed from the atmosphere. The top of envelope 29 must. alsobe sealed from the atmosphere and the preferred means toward this end is the application of a cap 39, which maybe made of glass and fits snugly in neck 3| of said envelope. The effectiveness of the sealed joint has been increased i by making neck 3| outwardly flared in form and member 21; (4) power transmission means 28 for producing relative motion between'holders25 and filling conduit member 21, which in this instance consists in rotating said member 21, the

by correspondingly tapering cap 39; also by pro viding ground mated surfaces. Incidentally, the reduced internal pressure will exert a tightening pull on cap 39 and alsoon receivers 26.

Cap 39 preferably is hollow and opens .downwardly into'the interior of envelope 29. In order to admit distillate samples from the valve-controlled drainage duct M of collector H of the dis- .tillationapparatus, extension duct 22, which leads downward therefrom, has beenjoined hermetically to thetop wall of cap 39 in such a manner that it projects into the interior of said cap to a point slightly eccentric to the axis of the latter to form a delivery spout 40. Branch line 23 of vacuum line 0' of the distillation apparatus also is hermetically joined to the top wall of cap 39 in communication with the interior of envelope 29 to insure complete equalization of pressure'between said envelope of the sample cutter and the interior of said distillation apparatus. This pressure equalization is necessary to permit flow of distillate from collector H into envelope 29 through drainage duct M, valve N, and extension duct 22.

Filling conduit member 21 is entirely located in the sealed interior of envelope 29 and cap 39 and is of such shape and size that it may be inserted freely through neck 3| at the time of assembly. By means to be described presently, filling conduit member 21 is mounted inside envelope 29 to rotate on a vertical axis concentric to the circular row of receiver holders 25. In construction, filling conduit member 21 preferably includes a funnel-shaped upper portion 4| having a mouth of such diameter that it underlies the spout 46 of drainage duct 22. A conduit 42 leads radially outward and downward from funned portion 4| to a discharge spout 43 which overhangs the circular row of holders 25. While filling conduit member 21 may be pivotally mounted in various ways, it is preferred to employ the vertically aligned upper and lower pintles 44 and 45, respectively, which project axially from said member 21 and are journaled in bearings and 41 provided respectively in the top wall of cap 39 and the bottom wall 33 of envelope, 29.

The advantage of locating filling conduit mem- -ber 21 and its pivotal bearings entirely inside sealedenvelope 29 is that there are no externally I exposed bearing faces to permit air fromthe atmosphere to leak into the envelope and thereby .upset the carefully established pressure condi- ,Due to the sealed-in condition of filling conduit member 21, propulsion, of said member is eflected by'magnetic attraction in penetration -member 21 adjacent to discharge spout 43 and of the bottom wall 33 of envelope 29. Magnetic means, which may be a permanent magnet 49, is affixed to the underside of filling conduit is of such form that its under face will move in a circular path closely adjacent to wall 33. Ad ditional magnetic means, which also maybe an exteriorly located -:permanent magnet $0, :for cooperation with interior magnet 451 is :aifixed -'.to a movable propelling-member preferably the ifnee end of a radiallyofiset arm :o'fdrivenshaftzfl,

which latter is 'rotatably -mounted on an axis coincident with the rotational axis of .filling -conduit member 21 in albearing:brackets53 supported by and extending irom standard Lulu-of supporting structure 24 beneath :envelope -29. "Magnet 55) 'isdisposed "with "its upper face closely adjacent to wall x33 and substantiallyequidistant 'withfmagnet 49 fromthecommonrotationalaxis, whereby, when both :magnets are .brought into close proximity to each-other, rotation of :driven shaft 52 will 'causepropelling member i l to move -in a path parallel-to the row of sample receivers and thereby produce concurrent rotation of fill- "injg "conduit member 2-'l. Shaft 52 is driven by magnet drive shaft 54, which is also journaled in bearing bracket 53, through the -medium of direction-change means such as beveled gears 155- 56.

Ma'gnet drive shaft *54 is diagrammatically represented in Figs. 4 to 8, inclusive, in operative cooperation with automatic means for -intermittent-1y rotating said shaft to move dischargespout 4'3 of filling conduit-memberfl by=step-by-step from one receiver holder to the next one with suitable dwell periods in holder-registering positionsto permit *the drainage of distillate samples i into "the *respective receivers.

Reierr-i-ng now=to Fig.4 in particular, the preferred form of electro-mechanical operating *meansfor-thesample cutterwill' now be described. Incidentally, this figureof =drawingrepresents in brok-en lines the operating means-in inoperative, shut down condition following .a completed major-cycl'e sample cutting 'run and requiring "the closing of a re-setting electric switch, which has just occurred, before further operation pan-commence. The prime mover for the operating means -isa constant-speed electric motor '51, which is connected with a source of current primarily "throughconductors 58- 59. A main switehifiil :controls :the connection of power circuit' 58 55 with the source.

Prime mover motor 51 causes rotation 'of a camshaft 6! Lin-counter-clockwise-:direction at veny' slow-speed.through the--medium=-of reduczti'on gearing (not shown). In the illustrative examplait will be assumed that. the speed isone .i evolution per minute. 'On-camshaftiH :there 81 611111338 CamaWhGBlS82y63 and 64,'wh-ich respectively actuate electricswitches- 65, 65 and-67.

Each of the three switches B5-666| may be efiany- 'desired type, -such-as a micro-switch for --:example, but is conventionally represented in whe -drawings :as comprising -a stationary contact :member Sit-and amovable contact member t9, awhich latter acts as a cam-follower in relation toiits corresponding cam wheel. Spring ll] serves "'both to pause movable contact -member 59 to -:-follow its cam .wheel and: toopen: the -switch.

:Gamwhee1 82 has a cam indentation Ji and a dwell surface 72 which extends throughout an arc Of'n9'l'1 y- 360 degrees. In :the operational scondition of the mechanism: represented-in Fig-:4, iswitchik'iii isropen and: cam indentation =11 is in ;position toclosessaid-switch as soonas-camshaft e81 :commences .to rotate. lFhereanfter,-. dwe1l-suriface 1 2 awillzkeepiswitch e8 5 closed Jahmushout a .completemevolutionpf camshaft Bl. Function- :ally. switch 65. is -a maintainerswitch.

Statio nary -,.contact .inember 6,8 ;and;.rnoyable :switch 1.5 will p rmi current to :fi we szs athe sea Timer 16 mayb of any wellilmown ype whichmayb set to cl se thecircuit of switch neith r atzp edet rm ned.tim intenrals or in response to changes .i temperature o yolume of the distillate t e motion-er- -pa-ratus as reg ster d by .recordine ermornetric .means or a liquid -level gauge, ;respectively not shown), operative ly ,associated with said .ap- .paratus. We do not'claim inventionof anything new the timer-or in its .specificoperational =relation to the distillation apparatus. ,O ir invention lies in the periodic energizationof the .mercury switch in order to start prime :mover motor 15'! automatically in -response to apredetermined COIldltlOIlz-Whillh it is desired shall initiate each minor-cycle of operation of thasamme cutter whichcauses the drainage of each distinct distillate cut or fraction intoone of thesample receivers and also causes,subseguentadyanceof thelfilling conduit member-into registration with the next succeedingsample receiver .of ,theefilies.

"Closing of switch 55 servesto ,additionallyolose the gap in conductor 59 of the power circuit, which otherwise would hoopened as -soo n.as mercuryswitch 35 becomes deeenergized at the end of the momentary starting irnpulse suppliegl thereto by timer 16. According to their o pel:- ational functions, mercury switch Tl5;is.,the,pri

mary starting switch andswitchfii is the primary maintainersWiGph.

Switch 66 is shown inopen condition withits movable contact ,member riding on fthe .dwel1 surfacel'l ofcam wheel This dwellsurface 11 extends through an .arc of substantially .180 degrees in orderto keep switchfiiopen throughout approximately one-half revolution of carn- ,,shaft 6!. .A cam face 78 of substantially degrees of arc .inextent intervenes between the .ends of dwell surface .ILand is adaptedtoact .upon movable contact member .69 in a manne to close switch .65 for the remaining One-half of ,the cyclic revolution of camshaft .61.. Cam face L8 is represented inLa position whereinit will Ibeoomeoperatively engaged with movable contact member 69 of switch .86 as soon as ca mshaft .61, commences to rotate.

SwitchBG serves vto controlthe electriccirquit of the solenoid coil oidrainage valve Not the distillation apparatus and maybe termed the drainage switch. To" this end, stationary contact member 58 and movab evco tact m mherifl are connected ,in parallel with power circuit ,58-59'by conductors-l9 andfifl, respectively. 'Cir- ,cuitj 22 of drainage valve N is connected in series with conductor T8. 'When switch fiii is closed, valve-N willjbe opened to permit drainage from collectonH to the sample cutter-2i of a sample out or fraction of the distillate in;;said collector. The volume of the cut will depend upon the closed condition time of switch6B-as-determined by the length of -can1--face i8 and the speed ot rotation'of camshaftfi l a Cam -wheelifl has a cam nose-8i and adwell surface :32 which extends through an .-.arc,of

;nearly ;36.0.degrees. :In the operational ;,condili n or .the mechani m epresented in E s- 2 switch 28 o ena c m;.no 8 .hasdu -.acontact;member 1590i switch ,fi5rarerconnectedn cleared movable :contact member $9 of .said

switch at the end of a preceding revolution of camshaft BI. Switch 61 is therefore open and will be maintained open by dwell surface 82 throughout nearly 360 degrees of rotation of camshaft 6|. Said switch 8! is connected in series with the starting power circuit 83 of the motor 84 which operates magnet drive shaft 54. Starting power circuit 83 is connected in parallel with main power circuit 58-59. When cam nose 8| of cam wheel 64 approaches the position shown in Fig. 4, which marks the end of a cyclic revolution of camshaft 6|, switch 61 will be closed momentarily to start magnet drive motor 84. Switch 61 thus constitutes a starting switch only and may be termed the secondary starting switch. Further operation of motor 84 is con tinued, until magnet drive shaft 54 has turned through a fraction of a revolution sufiicient to advance discharge spout 43 of filling conduit member 21 one step from a filled sample receiver to the next succeeding empty one, through the action of an intermittent-feed cam wheel 85 aifixed to said drive shaft. This feed cam wheel has plural, regularly spaced cam noses 88 with intervening dwell indentations 81 which are equal in number to the sample receiver holders 25 of sample cutter proper 2I. Fewer than the actual number of indentations are shown in Figs. 4 to 8 due to the reduced scale employed. A secondary maintainer switch 88 controls a secondary crcuit 89-83 for magnet drive motor 84, which is also connected in parallel with main power circuit 58-59. Said switch 88 comprises stationary contact member 98 and movable contact member 9|, which latter is urged by spring means 92 against the peripheral faces of intermittent-feed cam wheel 85. In the shut-down condition shown, feed cam wheel 85 is in midstep position, wherein switch 88 is closed, in the broken line representation.

When starting operation of magnet drive motor 84 occurs, through the closing of starting switch 67, intermittent-feed cam wheel 85 will be moved counter-clockwise in partial rotation sufficiently before said starting switch is opened again to effect closing of maintainer switch 88 under conditions represented in subsequent views wherein said switch 88 is in open position. In this way, continued operation of motor 84 is assured just long enough to advance intermittentfeed cam wheel 85 one complete step. When movable contact member 9| of switch 88 has dropped into the next indentation 81 of intermittent-feed cam wheel 85, the said switch will open the secondary circuit of motor 84. Movable contact member 9I additionally cooperates with the indentations 81 of said cam wheel 85 to provide a pawl-and-ratchet action which offers sufiicient resistance to motor 84 in its power-ofi condition to stop it instantly each time said movable contact member enters one of the indentations. A second cam wheel 93 on magnet drive shaft 54 cooperates with an automatic shut-down switch 94 to open the main power circuit upon completion of a major cycle of the sample cutter when the trailing sample receiver of the series has received its distillate cut. Said cam wheel 93 has a cam indentation 95 and a dwell surface 96 which extends throughout an arc of nearly 360 degrees. In the operational condition of the mechanism represented in solid linesin 4, shut-down switch 94 is closed as a result of previous closing of a reset switch which will be described more fully presently. Stationarycontact member 91 and spring-opened movable conthrough energization of circuit 89switch 88 circuit 83, and thereby effect completion of the advance of filling conduit member 21 from the trailing receiver holder 25 in the series to the leading one preliminary to the commencement of a new sample cutting run. This action is al most instantaneous and precedes any operation of prime mover motor 51. When completed, movable contact member SI of switch 88 will have dropped into the next indentation 81 of intermittent-feed cam wheel and said switch will have opened. At the same time, shut-down switch 94 will have been closed by movement ofcam wheel 93. Dwell surface 99 of cam wheel 93 will thereafter maintain switch 94 closed throughout the remainder of the intermittent major cycle one revolution of drive shaft 54.

During the major cycle of operation of the sample cutter, it is desired that distillate from the top of column A of the distillation apparatus shall be diverted into collector H at intervals in accordance with the time ratio established by a predetermined setting of timer T, whereas, upon termination of said major cycle, return of the.

distillation column A to a total reflux condition is imperative. These requirements have been met by providing a total reflux restoration switch I 92 for actuation by a third cam wheel I83 on magnet drive shaft 54. Stationary contact member I84 and spring-opened movable contact member I85 are connected in series with conductors 28-28 of the circuit J of electromagnet I, which actuates swinging funnel E of the distillation ap- 7 paratus and which is primarily controlled by timer T. When switch I82 is open, as shown in broken lines in Fig. 4, the circuit J will be open to permit swinging funnel E to assume its vertical total reflux position (not shown). Cam wheel I83 has a cam indentation I88 and a dwell surface I81 extending through an arc of nearly 360 degrees. In the operational condition represented in Fig. 4, cam indentation I 86 has just closed switch I82. Thereafter, dwell surface I81 serves to keep switch I82 closed throughout the remainder of one revolution of shaft 54 or until the end of the complete major cycle of operation of the sample cutter. f I

The operation of the preferred embodiment of the invention in cooperative combination with a reduced-pressure type distillation apparatus should be understood upon successive consideration of Figs. 1, 2, 4, 5,6, 7 and 8.

It will be assumed that the operator of the dis H tillation apparatus has returned to the laboratory and found everything in the expected conditiori following completion of an overnight major cyclic run of the sample cutter. All of the receivers 26 contain their respective cuts of distillate and are still attached in fluid-tight relation to holders 25. Cam-actuated switches 85, 68, 61, 94 and.I82 are open, but secondary maintainer switch 88 is closed. These positions of switches 88, 94 and I82 are represented in broken lines in Fig. 4 (and also in Fig. 8). The movable contact members of these switches have beenv foreshortened in I order to illustrate more clearlytheir major ycle terminal positions, which are slightly different from the solid line positions in Fig. 4, which represent. the condition after reset switch til-ll: has been closed manually to operate. magnet. drive motor 84 just long enough to shift discharge spout 43 of filling conduit member 2:'l- (Figs. 1 and 2) into registration with the-holder to which the first sample receiver of a new series is to be attached. Since closing of reset swtich iili:

would have no effect on. motor 8'4 if secondary V maintainer switch 88. were not closed at the time, by displacing the cam indentations 81' of intermittent-feed cam wheel 85 angularly from cam indentations 95 and W6, respectively, of cam wheels 93 and I03, one dwell surface 88 f. said cam. wheel 85 will be. pressing movable contact member 91 into circuit closing contact with stationary contact member 56: while movable: con-- tact members Stand H35, respectively, of switches Bland. ['82 are seated in circuit opening positions incamqindentations 95 and. WE, respectively, of calm wheels 93. and 103. as represented in broken lines.

Before the liquid-containing; receivers 25- can be detached from their respective holders 25 for. replacement by a freshseriesof. empty receivers, it is necessary to close valve 2%. and then open atmospheric vent valve 231; in order topreserve thevacuum condition in the distillation appara. tus and to release the suction on the: receivers. Valve N must be in closed condition, too, but that was effected automatically upon completion of .the final minor cyclic closing'operation of. switch 66.

When the fresh series ofempty sample receivers are in attached position and properly secured by devices 35, atmospheric vent valve 23b is closed and valve: 23a is then opened. Now, reset switch llll is closed momentarily to start magnet drive motor 84 and thereby turn. cam wheels 85-, 9:3 and. I03 tothe positions shown in solid: lines' in Fig: 4: It should now be realized why it. is soessential that secondary starting switch 88 be closed prior to the manual closing of reset switch 10!. Otherwise, the circuit 79-89-433 which connects magnet drive motor 84 in parallel with circuit B--5999--l00. would be open. At the instant reset switch llll is closed, circuit 20 will be closed. (live condition shown by heavy lines) by reflux. restoration switch I02 to make it possible for timer T of the distillation apparatus to commence. its. periodic operation of swinging funnel E through alternate energization and de-energization. of electromagnet I at the predetermined time. inter.- vals. With the exception of circuit 20, all other local circuits represented in Fig. dare dead (light lines) and allmovable parts of the mechanism are at. a standstill.

Turning. now to Fig. 5, it will .be-observed. that the first stage of the. first minor cycle of opera..- tionofthe sample cutter has occurred At this stage, timer 16. has energized the primary circuit of. mercury starting switch. '15 and this switch. has closed the circuit 58-59-9.9.--icllswitch 94 (heavy lines). to start prime mover motor 51-; Fig. 5 represents the condition at the instant motor 57 is about to start...

The energization period. of primary starting switch 15,. as established by timer I5, is sufficient to turn camshaft 61 counter-clockwise until primary maintainer switch 65 has become closed, as shown inFig. 6, to continue operation of motor 51. Drainagecontrol. switch 66 also has. been closed. to efiecttthe opening of solenoidv valve N of the distillation. apparatus and thereby start drainage of distillate from collector H down extension-1 duct 22 to filling conduit member 21.- This may be termed the primary drainage stage. Throughout substantially half a revolur tion of camshaft 6l-,.cam face 18 of cam wheel d! will. keep switch 6.6 closed. Thereafter, dwell surface 11 will permit switch 66 to open and-re..- main in that posit-ion for substantially another half revolution to permit drainage of the cut sample on down through filling conduit member 21- into the sample receiver aligned with its. discharge spout 43; This may be termed the: secondary drainage stage and is represented near.- ly at the end of its progress in Fig. 7. This view also shows secondary starting switch El closed momentarily by cam: nose ill of cam wheel. 64 to. start magnet drive motor 84. Said motor 84 has turned counter-clockwise sufficientlyto; close secondary maintainer switch 88: and thereby continue the operation of said motor until. filling conduit member: 2T has been advanced? one step from the filledreceiver to the next emptyreceiver' of the series.

Fig. 8 represents the condition of movable parts and. switches when filling conduit member 21 has: completed that step and marks'thc' end ofthe first minor cycle of operation. It hasbeen mentioned already that movable contact. mom.- bers- 9'8 and H35 of switches 9'4 and i102; respectively; are shown by broken lines: in the positions. which will be assumed at the end of a; major cycle. At that time, camshaft 54 will have com pleted one revolution and allsample receivers will have been subjected to the-service of filling conduit member 21.

It will be observed in Figs. 4 through E'that dwell surfaces 96' and 101' of cam wheels 93 and ms, respectively, serve to keep shut-down switch 94 and reflux restoration switch 102' closed throughout the entire major cycle. When shutdown switch 94 has been opened automatically at the end of the major cycle, the circuits of motors Hand 84 will be interrupted until reset switch llll is again manually closed to bring about the operational stage of Fig. 4. The complete major cycle incidental to one revolution of camshaft 54 requires as many minor cycles incidental to revolutions of camshaft 6! as there are sample receivers in the series (sixteen in the illustrative example).

Sometimes it becomes necessary to take one or more-sample cuts independently of a cyclic series run, either at a different time or during such a run but aperiodic in relation to the regular cuts of the major cycle. To meet this requirement, manual switches 28!) and 3%, respectively, have been provided in circuit B3'83. in parallel relation to secondary starting switch 61. and in, circuit l9-Bl! in parallel relation to switch 66. Momentary manual. closing of switch 200 will. start magnet drive motor 84 and, with the cooperation of secondary maintainer switch 88, continue operation of saidmotor until filling conduit member '2'! has been shifted into reg-- istration with an empty sample receiver in the applied series. Then, closing of switch 300 for an. appropriate length of time will cause drainage of the desired volume of distillate into thev selected receiver. If this be done after termination of a minor cycle but before the next periodic. energization of the operating circuit. of motor 51, the, irregular cut or cuts may be taken without affecting. continuity of the major cycle. Bee cause. of the usual elapse. of. several minutes-be.-

tweenpminor cycles, the interposition of casual samp e Guts is entirely practicable. If the re.-

13 ceivers which contain the casual cuts are to be removed at once for immediate test purposes, valves 23a. and 23b must be manipulated in the previously described manner before and after substitution of empty receivers for those whichcontain the casual cuts. The purpose of the substituted empty receivers is to seal the holders to which the receivers which were removed were attached. If the individual holders are provided with cut-off valves in accordance with the modification disclosed in Fig. 3, all that will be necessary is to close the cut-off valves of the affected holders.

Figs. 9 to 11 illustrate a modified form of sample cutter which is adapted for use with distillation apparatus that operates on the atmospheric distillation principle, or in connection with any apparatus which does not require sealing of the filling conduit member of the sample cutter from-v the atmosphere during delivery of sample cuts to the receivers. The modified sample-cutter is very much more simplified than the preferred form illustrated in Figs. 1 and 2, and is better suited to the cutting of samples of granular or pulverulent solid materials.

In this instance, supporting structure 24 supports a unitary receiver holder assembly I08, which is in the form of a hollow annular, body having individual holder sockets I in its top wall and is well adapted for utilization as a heatexchange tank whenever it is desired to modify the temperature of the samples delivered to sample receivers IIO mounted in said sockets. As usual, sockets I09 are arranged in a circular row. Each sample receiver I I0 has an enlarged mouth 0' which may rest upon the marginal edge of the holder socket in which it is inserted. (Fig. 10.) Enlarged mouth I I0 also serves as a manipulating portion which may be engaged by the operators fingertips to facilitate withdrawal from the socket. Furthermore, the mouth IIO' presents a seat for a preferably spherical sealing closure member III associated with each holder socket I09. (Figs. 9 and 11.) I

Holder assembly tank I08 is intended to contain a heating or cooling fluid agent, which may be supplied through bottom inlet H2 and discharged through elevated outlet I I3 which determines the surface level in the case of liquid agents. In use, sample receivers IIO will be immersed in the fluid agent so that the desired heating or chilling of their contents may take place.

The filling conduit member H4 differs slightly from that shown in Figs. 1 and 2. Instead of having rotational pintles, the portion I I5 located between funnel-shaped mouth I I6 and radially offset discharge spout II! is vertically disposed for engagement by an adjustable clamp II8 provided at the top of an extension piece H9 of driven shaft 52 of transmission mechanism 28.

Said transmission mechanism is the same as in the preferred embodiment of sample cutter, but driven shaft 52 is modified to provide for detachable connection of its upper end with extension piece II9. For convenience in permitting quick detachment of extension piece I I9 while producing concurrent rotation of said extension piece and driven shaft 52, the former has been provided with a terminal non-circular socket I20 for reception of the correspondingly shaped lower end I2I of the latter. In assembled position on extension piece II9, the vertical portion II5 of filling conduit member II4 will be centrally disposed in relation to the circular row of receiver .14 holder sockets I I 0 and discharge spout II I will be positioned to follow a circular path of movement overlying said holder socket row for sequential registration with the respective sample receivers IIO.

The spherical closure members III for the respective sample receivers are mounted to roll on track members I22, which are laid on the top wall of holder assembly tank I08 in horizontal alignment with the respective holder sockets I09. The track rails I2 2I22 of'track members I22 are inclined downward toward the corresponding holder sockets I09 and have laterally aligned check notches I22"-I22" which are intended to seat the respective closure members III in idle, inoperative positions spaced to the mouths IIO of receivers IIO when mounted in holder sockets I00. The closure members III will thus be checked or restrained in their idle positions until pushed forcibly out of notches I22"-I22" in the direction of the corresponding holder sockets I09, whereupon they will roll outward and drop into seated closing relation to the mouths III) of sample receivers I I0.

Convenient means for propelling closure members I II from their check seats along the tracks into seated relation to the receiver mouths, one at a time as filling conduit member H4 is advanced step-by-step along the row of receivers,

is the propelling arm I23 that projects radially from extension piece H9. This arm I23 is disposed in following relation to discharge spout I I! of filling conduit member II4 (considering the direction of rotation of the latter) and is just long enough and high enough to engage and sweep the spherical closure member I I I associated with each holder socket I09 from its restraining track notches I22"I22" down the track into seated relation to the receiver IIO mounted in said holder socket during the forward advance of said filling conduit member to the next receiver of the series. I

An upright finger I24 is provided on propelling arm I23 for contact with the rear side of filling conduit member H4 to serve as positive means for driving the latter in its circular path of movement. Clamp II8 could be tightened sufficiently' to insure effective driving of filling conduit member I I4, but it is desirable to maintain that degree of frictional engagement between said clamp and filling conduit member which will permit the latter to yield instead of becoming broken in-the' event that discharge spout II'I thereof encoun-' ters an immovable obstruction in its path. For

instance, back-lash in the power transmission mechanism 28 might cause retrograde movementof spout I I1 into collision with a closure member s I I I which has just been firmly seated in the path of movement of said spout.

- The modified form of sample cutter disclosed in Figs. 9, l0 and 11 is operated by the electroence of vacuum in the preferred embodiment disclosed in Figs. 1 and 2. I

Having thus described the invention, we claim: 1. In a sample cutter of the class described.

accuses afsealing envelope of non-magnetic material,hav-- mg. communication. with a vacuum: line;. plural sample. receivers arranged in a; horizontal. rowwith. upwardly open; mouths, receiver holdermeans to support each sample: receiver in; $0,113.. Inunication with the interior of said; envelope and in: sealed relation to. the. outside atmosphere; a; filling conduit member enclosed entirely with-- i112. said. envelope and having an intake mouth and a: discharge: spout, means also. entirely enclosediwithin said'envelope for movabl-y mounting: saidfilling conduit member in. a manner to cause the spout. thereof totravel along; a path. overlying. the row of receiver mouths, av drainage. duct penetrating; said. envelope in. hermeticah lyg sealed joint therewith and having its inner? endrmeregistration with. the intake mouth of the filling: conduit member to deliver sequential cuts of: material into; the same, and means to. operate the filling conduit member in, its path of movement, from one receiver toanother in suczcession. in such amanner that the. vacuum cnditiorr-within the envelope; is preserved throughout the receiver filling operatiomsa-id operating. means comprising. a propelling member movable outside theenvelope in. a. path parallel. to the of;samp-le, receivers-,and mutually attracting magnetic means aflixed to the filling conduit member; and the propellingmember respectively in. such; proximity to; the intervening envelope wall that movement of the propelling member will produce-concurrent movement of the filling conduit member in a manner to cause its discharge: spout: to follow the. row of sample receivers;

2.. A device for cutting; periodic test samples fromgardistillation apparatus having a distillatiomcolumnacollector; aductleading from said distillation. column to said collector, adjustable diversion means movable between operative and: inoperativepositionsand adapted when in. operative position to divert refiowing distillate. from the upper portion of said distillation column. through said duct into. the collector and when ininoperativeposition to permit total reflux of distillate. within said column, a timer device to shift said; flow diversion means from one of. said positions to the other, a drainage duct leading from said collector, and valve means controlling said drainage duct, said sample. cutting device comprising: plural sample re.-- ceivers, receiver holder. means adapted to. support said sample receivers in a row for sequential: introduction of distillate cuts; a. filling conduit' member having its open upper end. underlying-the drainage duct of said distillation. apparatus and, having a discharge spout arranged to overlie the row-of receivers; power means for. producing relative motion. between said receiver. holder. means and said filling conduit member ina. manner to move the discharge spout or the latter along the row of receivers; intermittent feed means for interrupting said relative motion for a predetermined drainage period upon. registration of the filling conduit member dis.- charge spout with each sample receiver in sequential order; and means responsive to movement. of thefilling conduit. member to actuate the timer device in a manner to render the distillate diversionmeans of the distillation apparatus inoperative. and thereby restore said. distillation apparatusl to. total reflux condition upon registration of the discharge spout of the filling conduit membenwiththelast sample receiver of. the series.

3. A sample cutting device as defined in claim 2, wherein meansds; provided toopen the drainageductcontrol valve means during said drains age period.

it An automatic device for cutting sequentiasamples; from a moving or stationary body of liquid or solidmaterial located in the containing; vessel of an associated apparatus having; a: drain-- ageduct controlled'by;valve'means, said samplecutting device-comprising: a. series of sample lie-- ceivers;v receiver holder means supporting: said sample receivers in acircular row a filling; C011?" duit' member rotatably mounted on. an axis con-- centric to the row of receivers and havingits open upper. end underlying the drainage ductoi theassociated apparatus andv having a discharge spout arranged to-traverse-a circular path; over lying the row of receivers; a drive shaft adapted. to make: one mao'or; cyclic revolution during; progressof the filling conduit member alongthe complete series of receivers; power transmission means connecting-'the-drive shaft with the filling conduit member; asecond shaft adapted to makeone minor: cyclic revolution incident to. registra.-- tion: of thefilling conduit member with 320111? ceiver of the series; a prime mover to rotate-saidsecond shaft at constant speed; primary starting means for commencing operation of the, prime mover at predetermined intervals corresponding in number to the receivers in the series; primary: maintainer means for continuing operation: of. the prime mover. for one complete revolution oi said second shaft; means operable by saidsecond shaft for opening the control valve means oi the drainage duct for a predetermined period; power.

1 means for rotating the driveshaft; secondary;

starting means operable by said secondshaft. to start rotation. of the drive shaft following completion of said drainage period; secondary-maintainer means for continuing operation of. the drive shaft; stopping means fortheprime mover. operable following actuation of the secondary maintainer means; intermittent feed means for interrupting operation of, the drive shaft upon arrival of the filling conduit member discharge spout in registration with each sample receiver of the series; and shut-down means operable automatically to suspend operation of said prime mover at the end of the major, cyclic revolution. of: the drive shaft.

5. An automatic sample cutting device as defined in claim. 4, whereinmanually operable. re-- set-means is providedfor restoring the operative condition of the primary starting means to com.- mence a new major cycle.

6.. An automatic sample cutting device as delined in. claim, 4, wherein manually operable means is provided for independent operation of Dower means. for the; drive shaft and the means for operating the drainage duct control valve means, whereby-a casual cut may be deliveredto a selected receiver out of the regular sequential. order.

7. An automatic device for cutting sequential samples from a moving. or. stationary body of liquid or. solid material located inthe. containing, vessel of an associated apparatus having a drain.- age duct controlled by electrical valve means. said samplecutting device comprising: a. series. of sample receivers; receiver holder means supporting said sample receivers in a circular r'ow;. a filling conduit member rotatably mounted on an. axis concentric to. the row of receivers and having its open upper end underlying the drain ageduct of. the. associated. apparatus and.hav-

7 log. a discharge spout. arranged. to. traverse a. cir- 17 cular path overlying the row of receivers; a drive shaft adapted to make one major cyclic revolution during progress of the filling conduit member along the complete series of receivers; power transmission means connecting the drive shaft with the filling conduit member; a camshaft adapted to make one minor cyclic revolut-ion incident to, the registration of the filling conduit member discharge spout with each receiver of the series; a main electric power circuit; a prime mover motor to rotate said camshaft at constant speed; a primary starting switch adapted when closed to connect said prime mover motor with said main power circuit; means for automatically closing said primary starting switch momentarily at predetermined intervals; a primary maintainer switch adapted when closed to continue the connection of the prime mover motor with the main power circuit; cam means operated by said camshaft for closing the primary maintainer switch when said camshaft commences to turn and for maintaining said switch closed until the end of each minor cyclic revolution of the camshaft; an electric circuit for said electric drainage duct valve of the associated apparatus, said circuit being connected in parallel to said main power circuit; a switch for said valve circuit; cam means operated by said camshaft to close said valve circuit switch during part of each minor cyclic revolution of the camshaft; an electric motor to operate the drive shaft at constant speed; a starting operating electric circuit for said drive shaft motor connected in parallel with the main power circuit; a secondary starting switch for said starting circuit; cam means operated by said camshaft to close said secondary starting switch at the end of each minor cyclic revolution of said camshaft; a maintainer electric circuit for said drive shaft motor connected in parallel to the main power circuit; a secondary maintainer switch in said maintainer circuit; intermittentfeed cam means operated by said drive shaft and adapted to close the secondary maintainer switch momentarily each time the drive shaft motor starts to rotate to permit partial rotation of said drive shaft sufficient to move the filling conduit member discharge spout from any sample receiver to the next one in the receiver series; a shut-down switch connected in series with the main power circuit; cam means operated by the drive shaft for opening said shut-down switch at the end of each major cyclic revolution of said drive shaft to suspend all operation of the sample cutting device, said shut-down switch cam means being adapted to maintain said shut-down switch closed throughout the remaining major portion of each complete major cyclic revolution of said drive shaft; the relative arrangement of the intermittent-feed cam means and the shut-down switch cam means being such that the secondary maintainer switch will be closed when the shutdown switch is open; and a manual reset switch connected in series with the main power circuit and in short-circuiting relation to the shut-down switch to permit manual advance of the fillin conduit member from the last sample receiver of the receiver series to the leading receiver thereof and also to render the sample cutting device operative again by closing the shut-down switch.

8. A sample cutter as defined in claim 1, said row of sample receivers being circular in arrangement, and bearing means located entirely within the sealing envelope in sealed relation to the outside atmosphere for mounting the filling conduit member for rotation on a vertical axis concentric to the row of sample receivers.

9. A sample cutter as defined in claim 8, said sealing envelope having a side wall of circular horizontal cross-section and an upthrust bottom wall of exteriorly concave form providing an external central concavity and an internal annular channel between said bottom and side walls; the sample receivers being supported with their mouths in communication with said annular channel; the discharge spout of the filling conduit member being mounted to travel through said annular channel; the propelling member being disposed within the external concavity of the bottom wall of the sealing envelope and mounted for rotation on a vertical axis coincident with that of the filling conduit member; and the magnetic means of the filling conduit member being carried by the discharge spout thereof through said annular channel.

THADDEUS R. MARCELL. CARTER, E. PORTER.

OTHER REFERENCES Article entitled Automatic vacuum take-off arrangement for fractional distillation by T. F.

Brown and K. F. Coles, Anal. Chem. 19, 935 (1947). 

